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分散固相萃取结合超高效液相色谱-串联质谱法同时测定柑橘中春雷霉素与噻霉酮残留
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安姣,康霞丽,杨秦,赵其阳,张耀海,王成秋,焦必宁 中国农业科学院/西南大学柑桔研究所农业农村部柑桔产品质量安全风险评估实验室(重庆)农业农村部柑桔及苗木质量监督检验测试中心 
基金项目:国家现代农业(柑桔)产业技术体系建设专项(CARS-26);柑橘中丙溴磷等高风险农药残留风险评估(GJFP2019012)
中文摘要:建立了分散固相萃取结合超高效液相色谱-串联质谱(DSPE/UPLC-MS/MS)同时测定柑橘中春雷霉素和噻霉酮残留的分析方法。柑橘全果和果肉分别以含0.5%甲酸和含0.5%氨水的乙腈-水(7∶3,体积比)溶液提取,经十八烷基硅胶(C18)净化上机,用Waters ACQUITY UPLC HSS T3 色谱柱分离。以0.2%甲酸水-甲醇为流动相进行梯度洗脱,多反应离子监测模式(MRM)扫描,以基质匹配标准曲线外标法定量。结果显示:目标化合物在0.5~200 μg/L质量浓度范围内线性关系良好(r2>0.999),检出限(LODs)为0.006~0.04 μg/kg,定量下限(LOQs)为5~10 μg/kg;加标回收率为73.4%~104%,相对标准偏差(RSD,n=6)为1.6%~9.6%。该方法易于操作,灵敏度高,适用于柑橘中春雷霉素和噻霉酮残留的同时检测。
中文关键词:分散固相萃取  超高效液相色谱-串联质谱  柑橘  春雷霉素  噻霉酮
 
Experimental Techniques and MethodsSimultaneous Determination of Kasugamycin and Benziothiazolinone Residues in Citrus by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Dispersive Solid Phase Extraction
Abstract:An analytical method was developed for the simultaneous determination of kasugamycin and benziothiazolinone residues in citrus by dispersive solid phase extraction/ultra performance liquid chromatography-tandem mass spectrometry(DSPE/UPLC-MS/MS).Citrus whole fruit and pulp were extracted with acetonitrile containing 0.5% formic acid and 0.5% aqueous ammonia-water(7∶3,by volume),respectively,then purified with octadecyl silica gel(C18) and separated on a Waters ACQUITY UPLC HSS T3 column by gradient elution with 0.2% aqueous formic acid-methanol as mobile phase,finally analyzed in multiple reaction monitoring(MRM) mode and quantified by matrix matched standard curve external standard method.Results showed that there were good linear relationships for the target compounds in the range of 0.5-200 μg/L with their correlation coefficients(r2) larger than 0.999.The limits of detection(LODs) and the limits of quantitation(LOQs) were in the concentration ranges of 0.006-0.04 μg/kg and 5-10 μg/kg,respectively.The spiked recoveries ranged from 73.4% to 104% with relative standard deviations(RSDs,n=6) of 1.6%-96%.With easy operation and high sensitivity,the method is suitable for the simultaneous determination of kasugamycin and benziothiazolinone residues in citrus.
Key Words:dispersive solid phase extraction  ultra performance liquid chromatography-tandem mass spectrometry  citrus  kasugamycin  benziothiazolinone
引用本文:安姣,康霞丽,杨秦,赵其阳,张耀海,王成秋,焦必宁.分散固相萃取结合超高效液相色谱-串联质谱法同时测定柑橘中春雷霉素与噻霉酮残留[J].分析测试学报,2020,39(3):358-364.
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